CN101439975B - Electric porcelain sintering method - Google Patents
Electric porcelain sintering method Download PDFInfo
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- CN101439975B CN101439975B CN2008102364026A CN200810236402A CN101439975B CN 101439975 B CN101439975 B CN 101439975B CN 2008102364026 A CN2008102364026 A CN 2008102364026A CN 200810236402 A CN200810236402 A CN 200810236402A CN 101439975 B CN101439975 B CN 101439975B
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Abstract
The invention relates to a method for firing electric porcelain, which comprises the steps of low-flame temperature rise, oxygenolysis, reduction, high-flame heat preservation and cooling, and is characterized in that in a weak reduction period of the reduction step, and the volume content of oxygen in a kiln is controlled to be between 1 and 5 percent. Breaking away from an idea behind the prior method for firing electric porcelain that the kiln can not contain any free oxygen in the weak reduction period, the method for firing electric porcelain keeps an oxidizing atmosphere in the kiln for certain time by adjusting the flow of the air and fuel gases in the kiln in the weak reduction period when firing the electric porcelain. Thus, instead of yellowing, the glaze of products achieves increased gloss and turns a little red and bright.
Description
Technical field
The invention belongs to the electric porcelain production field, especially a kind of electric porcelain sintering method.
Background technology
Fast development of Chinese economy, competition of the same trade is more and more fierce, make the user more and more higher to the specification of quality and the expection of product, thereby the product appearance difficult quality that causes electroceramics manufacturing firm to produce satisfies user's requirement, under the prerequisite of ensuring the quality of products, improve the visual appearance of electrotechnical porcelain product, satisfy user's demand, become an important directions of Future Development.
The calcining system of electroceramics is exactly the requirement of the flame properties of differing temps section when heating up in the sintering curve, so that successfully finish the task of burning till that each temperature section is born.Calcining system in the past can satisfy the qualitative performance requirements (as electric property, mechanical property, cold and hot performance) of product, and the technology of this calcining system is also ripe, and concrete calcining system is summarized as follows:
One, the little fire temperature rise period
This stage heat-up rate is slower, be warming up to 300 ℃ by room temperature, heat-up rate is 10 ℃/h-15 ℃/h, and carry out suitable insulation at indivedual material time points, to guarantee fully discharge of the intravital moisture content of base (comprising mechanical bond water, crystal water, planar water), reduce base substrate and phenomenons such as little fire cracking, fracture occur;
Two, the oxygenolysis stage
This stage comprises the stage of being rapidly heated and moderate heat holding stage, and is specific as follows:
The stage that is rapidly heated is warmed up to 980 ℃ from 300 ℃, and heat-up rate remains on 25 ℃/h-45 ℃/h;
The moderate heat holding stage is warmed up to 990 ℃ from 980 ℃, and this stage is guaranteeing under the situation of temperature-stable, making the volume content of oxygen in the kiln be controlled at 8%-12%;
Its purpose of burning till mainly is to get rid of water of constitution, realizes the oxidation of organism, carbon, the decomposition of carbonate and sulfide, crystal conversion;
Three, reduction phase (990 ℃-end fiery temperature)
This stage is divided into strong reduction period and weak reduction period, and wherein, strong reduction period is 990 ℃-1130 ℃; Weak reduction period be 1130 ℃-end fiery temperature.Its purpose of burning till mainly is to realize the decomposition of vitriol, and liquid phase forms and the dissolving solid phase, forms new crystalline phase and crystal growth, the fusion of glaze.Whole process mainly adopts reducing atmosphere, promptly according to the content of CO in the different steps control kiln in a certain scope, reach the purpose of burning till, generally speaking, include only CO and CO in this stage gasometry
2, whole process can not have oxidizing atmosphere, otherwise iron becomes the oxide compound of iron at high price again at a low price, makes the jaundice of porcelain base easily, and its heat-up rate generally is controlled at 10 ℃ of-20 ℃/h;
Four, high fiery holding stage ends fiery temperature spot insulation 1-2 hour, ends fiery temperature range: 1250 ℃～1300 ℃, this stage will be controlled the amount of wind and combustion gas well, and this stage does not allow in the oxygen existence of wandering about as a refugee;
Five, cooling stages
This stage be from burn till end when beginning to cool down room temperature till, whole process 30-45 consuming time hour.In this stage, the intravital liquid phase of base begins to be frozen into glassy phase by plastic state, and realizes crystal conversion, the variation of simultaneous weight, volume, void content, color, blank strength, hardness and the generation of distortion etc.
In sum, tradition is burnt till idea and is thought that can not there be the oxygen of wandering about as a refugee in weak reduction period in the kiln, otherwise causes the jaundice of product glaze easily.But adopt this traditional system, though its product can satisfy electric property, mechanical property and cold and hot performance etc., from appearance, electroceramics overglaze glossiness is not high, and the people is satisfied in addition.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of electric porcelain sintering method is provided, this electric porcelain sintering method adds the oxygen of wandering about as a refugee at weak reduction period, and the electroceramics glaze glossiness that is fired into is improved, and glaze is rubescent shinny.
The objective of the invention is to solve by the following technical programs:
This electric porcelain sintering method comprises little fire temperature rise period, oxygenolysis stage, reduction phase, high fiery holding stage and cooling stages successively, it is characterized in that the weak reduction period step in the described reduction phase is as follows:
1) at 1130 ℃～1190 ℃, the volume content of CO in the kiln is controlled at 1%-3%, furnace pressure is 4-6Pa, heat-up rate is 10 ℃/h～15 ℃/h;
2) when kiln temperature reaches 1190 ℃～1200 ℃, the volume content of CO in the kiln is controlled at less than 2%, furnace pressure is 4-6Pa;
3) ooze the oxygen operation then, ooze the oxygen operation and be divided into for three steps:
The first step is warming up to 1220 ℃ by 1200 ℃, and 1h-1.5h consuming time is controlled at 0.6-1.2% with the volume content of oxygen;
Second step was warming up to 1240 ℃ by 1220 ℃, and 1.5h-2h consuming time is controlled at 1.2-2.0% with the volume content of oxygen;
In the 3rd step, by 1240 ℃ of fiery to end temperature of intensification, 1.5h-2h consuming time is controlled at 2.0-3.2% with the volume content of oxygen, and ending fiery temperature range is 1250 ℃～1300 ℃, enters high fiery holding stage after the fiery to end temperature that heats up.
The above high fiery holding stage is to end fiery temperature spot insulation 1-2 hour, and the oxygen volume content is 0.6%-3.2% in the kiln.
Electric porcelain sintering method of the present invention has been broken and has been thought in traditional electric porcelain sintering method, at weak reduction period, the viewpoint that can not have the oxygen of wandering about as a refugee in the kiln, the weak reduction period that is burning till, by adjusting the flow of furnace air and combustion gas, make the oxidizing atmosphere that guarantees certain hour in the kiln, do not cause the jaundice of product glaze like this, can increase the Gloss of Glazes degree on the contrary, make glaze rubescent shinny simultaneously.
Embodiment
Below in conjunction with specific embodiment the present invention is done and to describe in further detail:
Embodiment 1
Electric porcelain sintering method specifically carries out according to following steps:
(1) the little fire temperature rise period
Kiln temperature is warming up to 300 ℃ by room temperature, and heat-up rate is 10 ℃/h;
(2) the oxygenolysis stage
This stage comprises the stage of being rapidly heated and moderate heat holding stage, and is specific as follows:
1) stage that is rapidly heated is warmed up to 980 ℃ from 300 ℃, and heat-up rate remains on 25 ℃/h;
2) the moderate heat holding stage is warmed up to 990 ℃ from 980 ℃, and this stage is guaranteeing under the situation of temperature-stable, making the volume content of oxygen in the kiln be controlled at 8%;
(3) reduction phase
Enter reduction phase when temperature reaches more than 990 ℃, wherein temperature is strong reduction period from 990 ℃ to 1130 ℃ process, and is strong reduction period 9-13 consuming time hour, and the volume content of CO in the kiln is controlled at 5%;
When reaching more than 1130 ℃, temperature enters weak reduction period, described weak reduction period, and 4 hours consuming time, be warmed up to 1200 ℃ by 1130 ℃, specific as follows:
1) at 1130 ℃～1190 ℃, the volume content of CO in the kiln is controlled at 1%, furnace pressure is 6Pa, makes heat-up rate remain on 10 ℃/h;
2) when kiln temperature reaches 1190 ℃～1200 ℃, the volume content of CO in the kiln is controlled at 0.6%, furnace pressure is 6Pa;
3) ooze the oxygen operation then, ooze the oxygen operation and be divided into for three steps:
The first step is warming up to 1220 ℃ by 1200 ℃, and 1h consuming time is controlled at 0.6% with the volume content of oxygen;
In second step, temperature is warming up to 1240 ℃ by 1220 ℃, and 1.5h consuming time by adjusting the air-fuel ratio coefficient, is controlled at 1.2% with the volume content of oxygen;
In the 3rd step, temperature is by 1240 ℃ of fiery to end temperature of intensification, 1h consuming time, and it ends fiery temperature is 1250 ℃, and the volume content of oxygen is controlled at 2.0%, enters high fiery holding stage after the fiery to end temperature that heats up.
(4) high fiery holding stage
High fiery holding stage is to end fiery temperature spot insulation 1 hour, and this stage will be controlled the amount of wind and combustion gas well, and the content of assurance oxygen is 0.6%.
(5) cooling stages
Finish high fiery holding stage and burn till end of a period, enter cooling stages, 30 hours consuming time of whole process until cool to room temperature.
Embodiment 2
Concrete electric porcelain sintering method in the present embodiment is as follows:
(1) the little fire temperature rise period
Kiln temperature is warming up to 300 ℃ by room temperature, and heat-up rate is 15 ℃/h;
(2) the oxygenolysis stage
This stage comprises the stage of being rapidly heated and moderate heat holding stage, and is specific as follows:
1) stage that is rapidly heated is warmed up to 980 ℃ from 300 ℃, and heat-up rate remains on 45 ℃/h;
2) the moderate heat holding stage is warmed up to 990 ℃ from 980 ℃, and this stage is guaranteeing under the situation of temperature-stable, making the volume content of oxygen in the kiln be controlled at 12%;
(3) reduction phase
Enter reduction phase when temperature reaches more than 990 ℃, wherein temperature is strong reduction period from 990 ℃ to 1130 ℃ process, and is strong reduction period 9-13 consuming time hour, and the volume content of CO in the kiln is controlled at 2%; Enter weak reduction period when kiln temperature reaches more than 1130 ℃, described weak reduction period is warmed up to 1200 ℃ by 1130 ℃, and is specific as follows:
1) at 1130 ℃～1190 ℃, the volume content of CO in the kiln is controlled at 2%, furnace pressure is 5Pa, makes heat-up rate remain on 12 ℃/h;
2) when kiln temperature reaches 1190 ℃～1200 ℃, the volume content of CO in the kiln is controlled at 1%, furnace pressure is 5Pa;
3) ooze the oxygen operation then, ooze the oxygen operation and be divided into for three steps:
The first step is warming up to 1220 ℃ by 1200 ℃, and 1.5h consuming time by reducing the air-fuel ratio coefficient, is controlled at 0.8% with the volume content of oxygen;
In second step, temperature is warming up to 1240 ℃ by 1220 ℃, and time 2h by adjusting the air-fuel ratio coefficient, is controlled at 1.5% with the volume content of oxygen;
In the 3rd step, temperature is by 1240 ℃ of fiery to end temperature of intensification, 1.5h consuming time, and it ends fiery temperature is 1280 ℃, and the volume content of oxygen is controlled at 2.5%, enters high fiery holding stage after the fiery to end temperature that heats up.
High fiery holding stage is to end fiery temperature spot insulation 1.5 hours, and this stage will be controlled the amount of wind and combustion gas well, and the content of assurance oxygen is 1%.
Finish high fiery holding stage and burn till end of a period, enter cooling stages, 30 hours consuming time of whole process until cool to room temperature.
Embodiment 3
Concrete electric porcelain sintering method in the present embodiment is as follows:
(1) the little fire temperature rise period
Kiln temperature is warming up to 300 ℃ by room temperature, and heat-up rate is 13 ℃/h;
(2) the oxygenolysis stage
This stage comprises the stage of being rapidly heated and moderate heat holding stage, and is specific as follows:
1) stage that is rapidly heated is warmed up to 980 ℃ from 300 ℃, and heat-up rate remains on 35 ℃/h;
2) the moderate heat holding stage is warmed up to 990 ℃ from 980 ℃, and this stage is guaranteeing under the situation of temperature-stable, making the volume content of oxygen in the kiln be controlled at 10%;
(3) reduction phase
Enter reduction phase when temperature reaches more than 990 ℃, wherein temperature is strong reduction period from 990 ℃ to 1130 ℃ process, and is strong reduction period 9-13 consuming time hour, and the volume content of CO in the kiln is controlled at 3%;
Enter weak reduction period when kiln temperature reaches more than 1130 ℃, described weak reduction period is warmed up to 1200 ℃ by 1130 ℃, and is specific as follows:
1) at 1130 ℃～1190 ℃, the volume content of CO in the kiln is controlled at 3%, furnace pressure is 6Pa, gradually reduces air-fuel ratio fine setting coefficient, makes heat-up rate remain on 15 ℃/h;
2) when kiln temperature reaches 1190 ℃～1200 ℃, the volume content of CO in the kiln is controlled at 1%, furnace pressure is 4Pa;
3) ooze the oxygen operation then, ooze the oxygen operation and be divided into for three steps:
The first step is warming up to 1220 ℃ by 1200 ℃, and time 1.2h by reducing the air-fuel ratio coefficient, is controlled at 1.2% with the volume content of oxygen;
In second step, temperature is warming up to 1240 ℃ by 1220 ℃, and time 2h by adjusting the air-fuel ratio coefficient, is controlled at 2.0% with the volume content of oxygen;
In the 3rd step, temperature is by 1240 ℃ of fiery to end temperature of intensification, 2h consuming time, and it ends fiery temperature is 1300 ℃, and the volume content of oxygen is controlled at 3.2%, enters high fiery holding stage after the fiery to end temperature that heats up.
High fiery holding stage is to end fiery temperature spot insulation 2 hours, and this stage will be controlled the amount of wind and combustion gas well, and the content of assurance oxygen is 3.2%.
Finish high fiery holding stage and burn till end of a period, enter cooling stages, 40 hours consuming time of whole process until cool to room temperature.
Embodiment 4
Concrete electric porcelain sintering method in the present embodiment is as follows:
(1) the little fire temperature rise period
Kiln temperature is warming up to 300 ℃ by room temperature, and heat-up rate is 14 ℃/h;
(2) the oxygenolysis stage
This stage comprises the stage of being rapidly heated and moderate heat holding stage, and is specific as follows:
1) stage that is rapidly heated is warmed up to 980 ℃ from 300 ℃, and heat-up rate remains on 30 ℃/h;
2) the moderate heat holding stage is warmed up to 990 ℃ from 980 ℃, and this stage is guaranteeing under the situation of temperature-stable, making the volume content of oxygen in the kiln be controlled at 9%;
(3) reduction phase
Enter reduction phase when temperature reaches more than 990 ℃, wherein temperature is strong reduction period from 990 ℃ to 1130 ℃ process, and 10 hours consuming time of strong reduction period is controlled at 3% with the volume content of CO in the kiln;
Enter weak reduction period when kiln temperature reaches more than 1130 ℃, described weak reduction period is warmed up to 1200 ℃ by 1130 ℃, and is specific as follows:
1) at 1130 ℃～1190 ℃, the volume content of CO in the kiln is controlled at 3%, furnace pressure is 6Pa, gradually reduces air-fuel ratio fine setting coefficient, makes heat-up rate remain on 11 ℃/h;
2) when kiln temperature reaches 1190 ℃～1200 ℃, the volume content of CO in the kiln is controlled at 0.5%, furnace pressure is 4Pa;
3) ooze the oxygen operation then, ooze the oxygen operation and be divided into for three steps:
The first step is warming up to 1220 ℃ by 1200 ℃, and time 1.3h by reducing the air-fuel ratio coefficient, is controlled at 0.8% with the volume content of oxygen;
In second step, temperature is warming up to 1240 ℃ by 1220 ℃, and time 1.6h by adjusting the air-fuel ratio coefficient, is controlled at 2.0% with the volume content of oxygen;
In the 3rd step, temperature is by 1240 ℃ of fiery to end temperature of intensification, 2h consuming time, and it ends fiery temperature is 1300 ℃, and the volume content of oxygen is controlled at 3.2%, enters high fiery holding stage after the fiery to end temperature that heats up.
High fiery holding stage is to end fiery temperature spot insulation 2 hours, and this stage will be controlled the amount of wind and combustion gas well, and the content of assurance oxygen is 1.2%.
Finish high fiery holding stage and burn till end of a period, enter cooling stages, 40 hours consuming time of whole process until cool to room temperature.
Embodiment 5
Present embodiment is with a 120m
3The drawer kiln be that example further specifies:
The sintering procedure of the strong reduction period in little fire temperature rise period, oxygenolysis stage and the reduction phase in the present embodiment is all identical with the interior parameters of kiln among the embodiment 1, weak reduction period at whole sintering procedure, when kiln temperature during at 1130 ℃～1190 ℃, the volume content of CO in the kiln is controlled at 2.5%, furnace pressure is 5Pa, the air-fuel ratio coefficient is 8.94-9.60, gradually reduces air-fuel ratio fine setting coefficient, makes heat-up rate remain on 10 ℃/h～15 ℃/h;
When reaching 1190 ℃-1200 ℃ in the kiln, ooze the oxygen operation in this stage:
At this moment, the combustion gas valve seat opening is 43%-46%; No. one time air-valve position aperture is 47%-52%; Furnace pressure (5 ± 1) Pa; The air-fuel ratio coefficient is 9.60-10.20, and kiln is totally seven districts, and the air-fuel ratio fine setting coefficient in each district is respectively 0.96,0.94,0.98,1,0.92,0.90,0.96.
When oxygen was oozed in preparation, at first Jiang Ge district air-fuel ratio fine setting coefficient reduced, and reduces 0.01 at every turn, observe simultaneously and respectively distinguish variation of temperature, if certain district's temperature descends, then should distinguish the fine setting coefficient and strengthen, respectively distinguish the given air-fuel ratio of actual mixing ratio=system/fine setting coefficient this moment.Each distinguishes adjusted air-fuel ratio coefficient: 0.90,0.92,0.94,0.96,0.88,0.86,0.90, the given air-fuel ratio of system's this moment is 10.28, and each is distinguished actual mixing ratio and is respectively: 11.42,11.17,10.94,10.71,11.68,11.95,11.42.The gasometry sampling spot is three points, establishes a point, each point gasometry result in the middle of every kiln car:
First point: the CO%=0.2; CO
2%=9.4; O
2%=1.0;
Second point: the CO%=0.2; CO
2%=9.6; O
2%=0.8;
Thirdly: CO%=0.2; CO
2%=9.0; O
2%=0.8.
From the analytical results of above gas volume percentage composition, each distinguishes atmosphere homogeneous, has satisfied the O of processing requirement
2=0.6%-1.2%.It is pointed out that combustion gas this moment valve seat opening is that 45%, air-valve position aperture is 53%, furnace pressure is 5Pa.
Next, preparation will be oozed oxygen and be continued to strengthen, its working method is the same state bright, when temperature reaches 1215 ℃-1225 ℃, combustion gas this moment valve seat opening is 45%, No. one time air-valve position aperture is 54%, furnace pressure is 5Pa, the given air-fuel ratio of system is 10.68, each distinguishes adjusted air-conditioning: 0.88,0.86,0.90,0.92,0.82,0.80,0.86, each is distinguished actual mixing ratio and is respectively: 12.14,12.42,11.87,11.61,13.02,13.35,12.42, and each point gasometry result:
First point: the CO%=0.2; CO
2%=9.6; O
2%=1.8;
Second point: the CO%=0; CO
2%=10.0; O
2%=1.6;
Thirdly: CO%=0.2; CO
2%=9.4; O
2%=1.8.
Above result satisfies the O of processing requirement
2=1.2%-2.0%.
Continue to regulate the air-fuel ratio coefficient, Dang Ge district actual mixing ratio is: 13.10,13.25,12.89,13.21,14.12,14.10,13.36 o'clock, and each point gasometry result following (below be the gas degree):
First point: the CO%=0; CO
2%=9.0; O
2%=2.6;
Second point: the CO%=0; CO
2%=9.2; O
2%=2.6;
Thirdly: CO%=0; CO
2%=9.0; O
2%=2.8.
Electric porcelain sintering method of the present invention broken thought in traditional electric porcelain sintering method at weak reduction period, the viewpoint that can not have the oxygen of wandering about as a refugee in the kiln, the weak reduction period that is burning till, by adjusting the flow of furnace air and combustion gas, make the oxidizing atmosphere that guarantees certain hour in the kiln, do not cause the jaundice of product glaze like this, can increase the Gloss of Glazes degree on the contrary, make glaze rubescent shinny simultaneously.
Claims (1)
1. an electric porcelain sintering method comprises little fire temperature rise period, oxygenolysis stage, reduction phase, high fiery holding stage and cooling stages successively, it is characterized in that the step of weak reduction period is as follows in the described reduction phase:
1) at 1130 ℃～1190 ℃, the volume content of CO in the kiln is controlled at 1%-3%, furnace pressure is 4-6Pa, heat-up rate is 10 ℃/h～15 ℃/h;
2) when kiln temperature reaches 1190 ℃～1200 ℃, the volume content of CO in the kiln is controlled at less than 2%, furnace pressure is 4-6Pa;
3) ooze the oxygen operation then, ooze the oxygen operation and be divided into for three steps:
The first step is warming up to 1220 ℃ by 1200 ℃, and 1h-1.5h consuming time is controlled at 0.6-1.2% with the volume content of oxygen;
Second step was warming up to 1240 ℃ by 1220 ℃, and 1.5h-2h consuming time is controlled at 1.2-2.0% with the volume content of oxygen;
In the 3rd step, by 1240 ℃ of fiery to end temperature of intensification, 1.5h-2h consuming time is controlled at 2.0-3.2% with the volume content of oxygen, and described to end fiery temperature range be 1250 ℃～1300 ℃, enters high fiery holding stage after the fiery to end temperature that heats up;
The fiery holding stage of described height is to end fiery temperature spot insulation 1-2 hour, and the oxygen volume content is 0.6%-3.2% in the kiln.
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| CN101811878B (en) * | 2010-02-26 | 2012-09-26 | 肖汉宁 | Method for sintering electric ceramic by using oxidizing flame |
| CN102951897B (en) * | 2012-11-17 | 2014-03-12 | 严增容 | High-voltage electric porcelain rapidly fired with waste porcelain and method |
| CN103382115B (en) * | 2013-07-24 | 2015-10-28 | 江苏南瓷绝缘子股份有限公司 | The method for cooking of electric porcelain blank |
| CN103396165B (en) * | 2013-07-24 | 2015-09-02 | 江苏南瓷绝缘子股份有限公司 | Rod insulator insulator semi-conducting glaze formula and its preparation method and application |
| CN106431352B (en) * | 2016-08-30 | 2019-01-25 | 中国西电电气股份有限公司 | A kind of strong reduction phase firing adjusting method of porcelain insulator |
| CN108046763B (en) * | 2017-12-07 | 2021-01-26 | 中国西电电气股份有限公司 | Sintering method for preventing high-temperature deformation of dry-method hollow porcelain bushing |
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Assignee: XI'AN XD HIGH VOLTAGE PORCELAIN INSULATOR CO., LTD. Assignor: China XD Electronic Corporation Contract record no.: 2012610000104 Denomination of invention: Electric porcelain sintering method Granted publication date: 20111109 License type: Exclusive License Open date: 20090527 Record date: 20120613 |